CN104087176B - The preparation method of nilox resin - Google Patents
The preparation method of nilox resin Download PDFInfo
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- CN104087176B CN104087176B CN201410358273.3A CN201410358273A CN104087176B CN 104087176 B CN104087176 B CN 104087176B CN 201410358273 A CN201410358273 A CN 201410358273A CN 104087176 B CN104087176 B CN 104087176B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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Abstract
The invention discloses a kind of preparation method of nilox resin, comprise the following steps: by rosin, solvent and catalyzer add in reactor, are progressively warming up to 150 DEG C ~ 200 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1300 watts ~ 1600 watts, disproportionation reaction 30 minutes ~ 40 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin; Wherein, described solvent is hexane, heptane, the one in the straight-chain paraffin of these three kinds of materials of octane or naphthenic hydrocarbon; Described catalyzer is palladium-carbon catalyst; Described rosin, the mass ratio of solvent and catalyzer is 1:0.5 ~ 1.5:0.01 ~ 0.02.Efficiency of pcr product of the present invention is high, and product color is more shallow, and palladium-carbon catalyst can be recycled, and has saved production cost.
Description
Technical field
The present invention relates to rosin deep process technology field, especially a kind of preparation method of nilox resin.
Background technology
The main component of rosin is for being C by molecular formula
20h
30o
2the compound of resinous acid composition, such resinous acid chemically reactive is strong, usually needs to carry out the process such as hydrogenation, disproportionation reaction with the rosin generating stabilization to it.Nilox resin is lower due to production cost, is mainly used in synthetic rubber, ABS resin, water-soluble pressure-sensitive tackiness agent, printing-ink, pigment dyestuff etc.
The preparation method of traditional nilox resin is: add palladium carbon catalyst by after rosin melting, disproportionation reaction 3 hours ~ 5 hours under the high temperature of 230 DEG C ~ 290 DEG C, the reacted palladium carbon catalyst of this method loses activity and can not recycle, and its production cost is higher.
Summary of the invention
The object of this invention is to provide a kind of preparation method of nilox resin, this method can solve the high problem of production cost.
In order to solve the problem, the technical solution used in the present invention is:
The preparation method of this nilox resin, comprise the following steps: by rosin, solvent and catalyzer add in reactor, are progressively warming up to 150 DEG C ~ 200 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1300 watts ~ 1600 watts, disproportionation reaction 30 minutes ~ 40 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin; Wherein, described solvent is hexane, heptane, the one in the straight-chain paraffin of these three kinds of materials of octane or naphthenic hydrocarbon; Described catalyzer is palladium carbon catalyst; Described rosin, the mass ratio of solvent and catalyzer is 1:0.5 ~ 1.5:0.01 ~ 0.02.
In technique scheme, technical scheme is more specifically: described catalyzer is palladium carbon catalyst; Described rosin, the mass ratio of solvent and catalyzer is 1:0.8 ~ 1:0.025.
Owing to have employed technique scheme, the present invention compared with prior art has following beneficial effect:
Rosin is dissolved in solvent by the present invention, then adds palladium carbon catalyst, and passes into ultrasonic wave in reactor, and make reaction at a lower temperature with the disproportionation reaction of speed generation faster, side reaction is few, and efficiency of pcr product is high, and product color is more shallow; And in reaction process, palladium carbon catalyst activity is still good, can recycle, save production cost largely.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
By 100 grams of rosin, 150 grams of hexanaphthenes and 1.5 grams of palladium carbon catalysts add in reactor, are progressively warming up to 150 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1300 watts, disproportionation reaction 40 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
Embodiment 2
By 1 kilogram of rosin, 0.5 kilogram of heptane and 10 grams of palladium carbon catalysts add in reactor, are progressively warming up to 200 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 14500 watts, disproportionation reaction 35 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
Embodiment 3
By 10 kilograms of rosin, 10 kilograms of octanes and 0.2 kilogram of palladium carbon catalyst add in reactor, are progressively warming up to 180 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1600 watts, disproportionation reaction 30 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
Embodiment 4
By 100 grams of rosin, 150 grams of suberane and 1.5 grams of palladium carbon catalysts add in reactor, are progressively warming up to 155 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1300 watts, disproportionation reaction 40 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
Embodiment 5
By 1 kilogram of rosin, 0.5 kilogram of cyclooctane and 10 grams of palladium carbon catalysts add in reactor, are progressively warming up to 190 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 13500 watts, disproportionation reaction 35 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
Embodiment 6
By 10 kilograms of rosin, 10 kilograms of hexanes and 0.2 kilogram of palladium carbon catalyst add in reactor, are progressively warming up to 170 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1500 watts, disproportionation reaction 33 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
Claims (6)
1. the preparation method of a nilox resin, it is characterized in that comprising the following steps: by 100 grams of rosin, 150 grams of hexanaphthenes and 1.5 grams of palladium carbon catalysts add in reactor, are progressively warming up to 150 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1300 watts, disproportionation reaction 40 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
2. the preparation method of a nilox resin, it is characterized in that comprising the following steps: by 1 kilogram of rosin, 0.5 kilogram of heptane and 10 grams of palladium carbon catalysts add in reactor, are progressively warming up to 200 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 14500 watts, disproportionation reaction 35 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
3. the preparation method of a nilox resin, it is characterized in that comprising the following steps: by 10 kilograms of rosin, 10 kilograms of octanes and 0.2 kilogram of palladium carbon catalyst add in reactor, are progressively warming up to 180 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1600 watts, disproportionation reaction 30 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
4. the preparation method of a nilox resin, it is characterized in that comprising the following steps: by 100 grams of rosin, 150 grams of suberane and 1.5 grams of palladium carbon catalysts add in reactor, are progressively warming up to 155 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1300 watts, disproportionation reaction 40 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
5. the preparation method of a nilox resin, it is characterized in that comprising the following steps: by 1 kilogram of rosin, 0.5 kilogram of cyclooctane and 10 grams of palladium carbon catalysts add in reactor, are progressively warming up to 190 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 13500 watts, disproportionation reaction 35 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
6. the preparation method of a nilox resin, it is characterized in that comprising the following steps: by 10 kilograms of rosin, 10 kilograms of hexanes and 0.2 kilogram of palladium carbon catalyst add in reactor, are progressively warming up to 170 DEG C, and in reactor, pass into the ultrasonic wave that frequency is 1500 watts, disproportionation reaction 33 minutes; Filter, gained filtrate is vacuumized distillation, obtains nilox resin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410358273.3A CN104087176B (en) | 2014-07-25 | 2014-07-25 | The preparation method of nilox resin |
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| CN201410358273.3A CN104087176B (en) | 2014-07-25 | 2014-07-25 | The preparation method of nilox resin |
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| CN104087176A CN104087176A (en) | 2014-10-08 |
| CN104087176B true CN104087176B (en) | 2016-03-02 |
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| CN201410358273.3A Active CN104087176B (en) | 2014-07-25 | 2014-07-25 | The preparation method of nilox resin |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106085242A (en) * | 2016-06-26 | 2016-11-09 | 广西众昌树脂有限公司 | The preparation method of disproportionated rosin |
| CN106349937A (en) * | 2016-08-25 | 2017-01-25 | 广西兴业县新贵松脂厂 | Production method of high-quality disproportionated rosin |
| CN106349938A (en) * | 2016-08-29 | 2017-01-25 | 广西梧州通轩林产化学有限公司 | Method for preparing disproportionated rosin for hot-melt adhesive |
| CN109777301B (en) * | 2019-02-27 | 2021-03-30 | 广西创跃化工有限公司 | Preparation method of disproportionated rosin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0572680A1 (en) * | 1991-12-21 | 1993-12-08 | Arakawa Kagaku Kogyo Kabushiki Kaisha | Process for producing rosin ester and colorless rosin |
| CN1156745A (en) * | 1996-10-04 | 1997-08-13 | 张运明 | High-production low-consumption process flow for producing resin 731D |
| CN102127369A (en) * | 2010-12-16 | 2011-07-20 | 广东科茂林产化工股份有限公司 | Method for preparing disproportionated rosin |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100366692C (en) * | 2006-05-26 | 2008-02-06 | 广西民族大学 | Method for synthesizing maleated rosin rapidly |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0572680A1 (en) * | 1991-12-21 | 1993-12-08 | Arakawa Kagaku Kogyo Kabushiki Kaisha | Process for producing rosin ester and colorless rosin |
| CN1156745A (en) * | 1996-10-04 | 1997-08-13 | 张运明 | High-production low-consumption process flow for producing resin 731D |
| CN102127369A (en) * | 2010-12-16 | 2011-07-20 | 广东科茂林产化工股份有限公司 | Method for preparing disproportionated rosin |
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